Potassium Acetate → HCID 178494125, Verbindung

HRID 706002Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 706002
Cl.[Cl:2][C:3]1[CH:20]=[CH:19][C:6]([O:7][C:8]2[CH:13]=[CH:12][C:11]([CH2:14][CH2:15][C:16](=[NH:18])[NH2:17])=[CH:10][CH:9]=2)=[CH:5][C:4]=1[C:21]([F:24])([F:23])[F:22].[OH:25][CH:26]=[C:27]([CH2:32][C:33]1[CH:34]=[N:35][C:36]([O:39][CH3:40])=[N:37][CH:38]=1)[C:28](OC)=O.C([O-])(=O)C.[K+]>C1(C)C=CC=CC=1>[Cl:2][C:3]1[CH:20]=[CH:19][C:6]([O:7][C:8]2[CH:13]=[CH:12][C:11]([CH2:14][CH2:15][C:16]3[NH:17][CH:28]=[C:27]([CH2:32][C:33]4[CH:34]=[N:35][C:36]([O:39][CH3:40])=[N:37][CH:38]=4)[C:26](=[O:25])[N:18]=3)=[CH:10][CH:9]=2)=[CH:5][C:4]=1[C:21]([F:22])([F:23])[F:24]

Komponenten

5

Edukt 3

HCID 517044Potassium AcetateHCID 67773588Methyl 3-hydroxy-2-((2-methoxypyrimidin-5-yl)methyl)acrylateHCID 677756383-(4-(4-Chloro-3-(trifluoromethyl)phenoxy)phenyl)propanimidamide hydrochloride

Produkt 1

HCID 178494125HCID 178494125, VerbindungAusbeute 42,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

The suspension of 3-(4-(4-chloro-3-(trifluoromethyl)phenoxy)phenyl)propanimidamide hydrochloride (5.9 g, 15.56 mmol), methyl 3-hydroxy-2-((2-methoxypyrimidin-5-yl)methyl)acrylate (3.49 g, 15.56 mmol) and potassium acetate (4.58 g, 46.7 mmol) in toluene (100 mL) was heated under reflux overnight. Dean-Stark apparatus was used to remove water formed in the reaction. The residue was recrystallized in ethyl acetate and washed with ether to provide the title compound (3.4 g, 42%). LCMS: rt=1.71 min, [M+H+]=517

Aufarbeitung

  1. temperaturewas heated
  2. temperatureunder reflux overnight
  3. customto remove water
  4. customformed in the reaction
  5. customThe residue was recrystallized in ethyl acetate
  6. washwashed with ether

Quellen und Nachweise

ORD-Eintrag
ord-aa43a47642d940aba5bc945523f33e5b
Quelldatensatz
uspto-grants-2015_11
Patentnummer
US09174968B2

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